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    30 August 2011, Volume 31 Issue 4 Previous Issue    Next Issue
    研究报告
    Preparation of Epoxy Resins from Fractionated Acetic Acid Lignin
    FENG Pan;CHEN Fan-geng
    2011, 31 (4):  7-12. 
    Abstract ( 1259 )   PDF (1102KB) ( 624 )   Save
    Acetic acid lignin (AAL) was fractionated into three fractions with different relative molecular mass at different concentration of acetic acid-water solution. These three fractions further reacted with phenol and yielded the corresponding phenolized lignins (PL). PL showed higher phenolic hydroxyl than that of AAL. Three kinds of lignin-based epoxy resins (PLEP) were prepared from PL by reacting with epichlorohydrin. PLEP showed the highest epoxy value(1.69 mmol/g), thermal degradation temperature (256.3 ℃),and the lowest char yield (41.6 %) using PL with the lowest relative molecular weight. It was found that the adhesive shear strength of the cured blends of PLEP and E-44 epoxy resin was improved compared with E-44 epoxy resin. For example, the cured blend of E-44 epoxy resin and PLEP prepared from PL with the lowest relative molecular mass showed high adhesive shear strength(7.9 MPa).
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    Energy-saving and Economic Assessment for Continuous Pipeline Porduction of Biodiesel
    NIE Xiao-an;CHANG Xia;ZHANG Tian-jian;CHEN Jie;LI Ke
    2011, 31 (4):  13-18. 
    Abstract ( 914 )   PDF (1134KB) ( 805 )   Save
    The energy-saving for continuous pipeline process with capacity of 1 000 t/a was analyzed. According to the pilot data, the energy consumption of continuous pipeline process for biodiesel production was discussed.It was found that the reaction time was greatly reduced from two hours to twenty minutes by co-solvent technology compared with the traditional method. The reaction period was greatly reduced, and the safety of production process was improved. The total energy consumption as equivalent standard coal was reduced from 28.669 kg/t by kettle process to 22.94 kg/t by pipeline process. The ratio of energy saving was about 20 %. The net profit for prodution of biodiesel was 258.68 yuan/t after tax refund. This pipeline technology has great prospect in industrial application.
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    Preparation and Application for Kaempferol Molecularly-imprinted Polymers
    YU Lan-zhe;QU Dan;YUN Yan-bin
    2011, 31 (4):  19-24. 
    Abstract ( 1396 )   PDF (1189KB) ( 683 )   Save
    A molecularly-imprinted polymer(MIP) was prepared by bulk polymerization, using kaempferol as the template molecule, 4-vinyl pyridine as the functional monomer, and ethylene glycol dimethacrylate as the cross-linker in the solvent system of CHCl3-DMF(3∶1, volume ratio). The synthesized polymer, i.e.kaempferol-MIP, was analyzed by FT-IR and scanning electron microscopey(SEM). In addition, the adsorption properties and mechanism were studied as well. The experimental results showed that the kaempferol-MIP exhibited a favorable affinity for kaempferol. The Scatchard analysis reveals that there exists a class of homogenous recognition sites in kaempferol-MIP within the range of certain concentration. Apparent maximal combination amount (Qmax) and equilibrium dissociation constant (KD) were calculated to be 3 938 μg/g and 9.074 mg/L, respectively. The result of selectivity study showed that the selectivity coefficient is 3.24 with respect to kaempferol-rutin system.
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    Experimental Investigation of Spray Droplet Size Distribution Using a Spinning Disk Atomizer
    HUANG Li-xin;WANG Chun-peng;ZHOU Rui-jun;XIE Pu-jun;MUJUMDAR A S
    2011, 31 (4):  1-6. 
    Abstract ( 1319 )   PDF (526KB) ( 709 )   Save
    Spinning disk atomizer is a key part in many spray drying systems. Few works exist in the literatures dealing with size distribution and changes of the droplets produced by such a type of atomizer. In this work, a model atomizer is used to spray-dry a re-dispersible glue emulsion on an industrial scale production 2 000 t/a. The maximum spray capacity of such an atomizer is 2 000 kg/h. The disk tested has a diameter of 180 mm and 24 channels. A laser analyzer was used to measure the droplet size distribution of sprays produced by the spinning disk atomizer. The effects of the disk rotating speed on water droplet size distribution were investigated. The rotating speed of the disk was varied from 16 000 to 10 000 r/min using a frequency-inverter. In order to investigate the change of droplet size to dried particle size from the spray dryer, the droplet size distribution of the re-dispersible glue emulsion and the dried particle size distribution produced were measured. The results show that the mean size was reduced from 92 μm of droplets to 72 μm of dried particles. It was also observed that the maximum dried particle size was larger than that of droplets due to droplet and particle agglomeration taking place within the spray drying chamber.
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    Production of Renewable Liquid Fuel by Catalytic Cracking of Soybean Oil
    CHEN Jie;JIANG Jian-chun;XU Jun-ming;NIE Xiao-an
    2011, 31 (4):  25-30. 
    Abstract ( 889 )   PDF (648KB) ( 766 )   Save
    Three types of triglyceride cracking processes i.e. batch process, rotating cone process and distillation process was studied. Several kinds of catalysts were compared with each other. It was found that the optimum reaction conditions are as follows: mass fraction of catalyst 5%, distillation temperature 320-350 ℃, cracking temperature 460-480 ℃ and feed rate 35 g/h. The fraction distribution of product was modified using alkalinic catalyst such as Na2CO3 and distillation process. From the results of FT-IR, GC-MS and SEC measurements, the products were determined to be consisted of alkanes, alkenes and carboxylic acids with carbon chain below C24 and lower average molecular weight. The physical and chemical properties of products were also detected to be close to those of petroleum-based fuels.
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    Synthesis of N-(2-Hydroxy-benzyl)-dehydroabietylamine and Its Corrosion Inhibition Properties on Carbon Steel in Hydrochloric Acid Solution
    HUANG Dao-zhan;LAN Hong-yun;LEI Fu-hou;LUO Li;WANG Xiao-shu
    2011, 31 (4):  36-40. 
    Abstract ( 1070 )   PDF (1127KB) ( 773 )   Save
    N-(2-Hydroxy-benzyl)-dehydroabietylamine (DARS) was synthesized through condensation of dehydroabietylamine and salicylaldehyde and followed by reduction using NaBH4. The structure of DARS was characterized by IR, UV and 1H NMR. Its corrosion inhibition behavior on carbon steel (type A3) in HCl solution was studied by weight-loss measurement and polarization curves. Due to secondary amino group in DARS sturcture, DARS displays better solubility and stability than DAS in HCl solution. Under conditions of 5.84% HCl solution with 0.005 % DARS at 40 ℃, the corrosion rate and corrosion inhibition efficiency on carbon steel were 2.5 g/(m2·h) and 98 % respectively. Polarization curves reveal that DARS is an absorb-type corrosion inhibitor.
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    Synthesis and Characterization of Ethyl Cellulose Monoester of Maleic Acid
    MO Ya-li;CHEN Ri-qing;WANG Chun-peng;BU Hong-zhong;CHU Fu-xiang
    2011, 31 (4):  31-35. 
    Abstract ( 961 )   PDF (1876KB) ( 642 )   Save
    In order to improve the use of ethyl cellulose, ethyl cellulose monoester of maleic acid was synthesized using ethyl cellulose as raw material and maleic anhydride as derivatization reagent. Its structure and properties were measured using Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and so on. According to single factor experimental results, the optimal experimental conditions were as follows: the molar ratio of maleic anhydride to the hydroxyl content of EC 4∶1, reaction time 6 h, the molar ratio of catalyst (anhydrous sodium acetate) to maleic anhydride 1∶1, reaction temperature 80 ℃. The product's degree of substitution (DS) is 0.41.The product can not only be used for graft copolymerization, but also can be used for crosslinking reaction.
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    Influence of Activated Carbon Microstructure on Decoloration Performance of Xylitol Solution
    JIAN Xiang-kun;LIU Shi-cai;BIAN Yi;DENG Xian-lun
    2011, 31 (4):  41-45. 
    Abstract ( 977 )   PDF (962KB) ( 722 )   Save
    Adsorption performance and microstructure were studied using four different sawdust activated carbons. It was indicated that the adsorption value of methyleneblue had great effect on the activity of activated carbons for decoloring xylitol solution. However, it was not the only factor. The number of activated carbons' mesopores, especially the size range of 2-14 nm, impacted greatly the decoloration performance of xylitol solution. The FT-IR analyses of the activated carbons showed that the presence of surface C—O functionality might promote the adsorption.
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    Effect of Activator Dosage on Pore Structure and Electrochemical Properties of Bamboo-based Activated Carbon
    CHEN Ming-zhu;LIU Hong-bo;ZHANG Dong-sheng;DENG Cong-jing;XIA Xiao-hong;HE Yue-de
    2011, 31 (4):  63-68. 
    Abstract ( 1079 )   PDF (1795KB) ( 691 )   Save
    Activated carbon with distinct pore structure used for electric double-layer capacitor (EDLC) was prepared using bamboo char as raw material and KOH as activator by chemical activation. The effect of mass ratio of KOH/carbon on the structure and properties of the activated carbon were investigated by means of SEM, nitrogen adsorption, galvanostatic charging/discharging, cyclic voltammetry and impedance spectroscopy. The results show that the BET surface area, the totle pore volume, mesoporosity volume and micropore volume of activated carbons increase firstly and decrease afterward with increasing ratio of KOH/carbon, while the average pore size increases all the time. The specific surface area, total pore volume and average pore size of bamboo-based activated carbon at the mass ratio of KOH/carbon 6 (BAC6) are 3 166.5 m2/g, 2.023 cm3/g and 2.555 nm, respectively. Meanwhile BAC6 exhibites excellent specific capacitance over 172.9 F/g at 1 mA/cm2 and the capacitance maintenance achieves 65.6 % at 50 mA/cm2 in organic electrolyte. The high current charge/discharge performance is improved by a reasonable mesoporosity and somewhat wide pore size distribution.
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    Synthesis and Structural Characterization of the Plasticizer Tri-lauryl Maleopimarate
    WANG Chun-ping;LEI Fu-hou;LI Hao;LI Peng-fei;HOU Wen-biao;JIANG Wen-duo
    2011, 31 (4):  46-52. 
    Abstract ( 987 )   PDF (1342KB) ( 624 )   Save
    The plasticizer tri-lauryl maleopimarate was synthesized from maleopimaric acid (MPA) and lauryl alcohol using p-toluenesulfonic acid as catalyst and n-octane as water entrainer. The optimal synthesis conditions were as follows: n(MPA)∶n(lauryl alcohol)1∶5, catalyst dosage(3.6 % of mass MPA), the water entrainer n-octane 15 mL, reaction time 8 h, reaction temperature 200-210 ℃ under nitrogen atmosphere. The contents of tri-lauryl maleopimarate reached 99.14 % by HPLC. The structure of tri-lauryl maleopimarate was characterized by FT-IR, 1H NMR and 13C NMR respectively. The molecular formula of tri-lauryl maleopimarate determined by elementary analysis was C60H106O6. The properties of the product were as follows: acid value 0.98 mg/g,heat weight loss 0.08 %, volume electric resistivity 2.6×1011Ω·m, open-cup flashing point 269 ℃, freezing point -55 ℃, density 0.980 g/cm3, index of refraction 1.484 6, moisture content ≤0.08 %, viscosity 0.200 Pa·s, respectively. TG-DSC curve of product was also measured. The results confirmed that it could satisfy the requirements of plasticizer.
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    Extraction Technology of Polysaccharide from Zizyphus jujuba by Ultrasound-assisted Enzymatic Method
    SUN Xiao-rui;WANG Na;XIE Xin-hua;LEI Dan;ZHANG Han-rui;CHANG Jun-xiao;AI Zhi-lu
    2011, 31 (4):  58-62. 
    Abstract ( 861 )   PDF (841KB) ( 715 )   Save
    The polysaccharide from Zizyphus jujuba was extracted by ultrasound-assisted enzymatic method. Its optimum conditions were investigated by the orthogonal design. According to the purity and extraction rate,the extraction effect of papain which was selected among papain, trypsin and neutral protease was better. The extraction conditions of polysaccharide by papain were studied. Finally, the optimum technological conditions of polysaccharide from Z. jujuba are as follows: material 10 g, the ratio of solid to liquid 1∶8, temperature 60 ℃, ultrasonic time 25min, ultrasonic power 70 W, after the ultrasound treatment, papain amount 0.15 %, pH value 6.0, enzymolysis time 120 min and temperature 60 ℃.Under these conditions, extraction two times,the yield of the polysaccharide was 21.95 %, the purity was 13.05 %.
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    Quality Variation during the Processing of Ya'an Tibet Tea
    CHEN Chang-hui;GUO Jin-long;WANG Yan-xia;DU Xiao;ZHAO Tao;ZHAO Zheng-lai
    2011, 31 (4):  69-74. 
    Abstract ( 1036 )   PDF (1122KB) ( 970 )   Save
    The variation of quality components during the processing of Ya'an Tibet tea was investigated. The results showed that the water content decreased with the processing. During the first 3 days fermentation, water content decreased the least and water loss was 3.01 %. During other stage, water content decreased at high level. During the 1-3 days fermentation, the temperature of the middle part significantly increased 24.40 ℃, while the temperature of the top part and the bottom part decreased. During the 6-9 days fermentation, the temperature is kept steadily. From leaves to product, the contents of catechin, tea polyphenols, caffeine, free amino acid and soluble sugar decreased 69.88 %、 46.39 %、 68.53 %、 25.85 % and 7.11 %, respectively. The content of total chlorophyll decreased 48 % while the contents of the TR, TF and TB increased 24.33 times, 53 times and 5.67 times respectively. Apparently, the quality components of Ya'an Tibet tea change fast during fermentation, and the temperature and humidity influenced it significantly.
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    Properties of the Cured Water-soluble Modified Amine from Fatty Acid Methyl Esters of Tea Oil Soapstock
    LI Mei;XIA Jian-ling;HUANG Kun;LIAN Jian-wei
    2011, 31 (4):  53-57. 
    Abstract ( 1010 )   PDF (885KB) ( 588 )   Save
    The effects of the diameter and viscosity of epoxy resin dispersion, the molar ratio of epoxy group to amino hydrogen and the curing temperature on the properties of the cured water soluble modified amine from fatty acid methyl esters of tea oil soapstock were investigated by thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), mechanical pro-perty test and scanning electron microscopy (SEM). It was shown from the results that the thermal stability of the cured film from the water-soluble modified amine CA-921 and the epoxy emulsion AB-EP-20 with smaller particle size and lower viscosity was better. When the water-soluble modified amine CA-921 cured with the epoxy emulsion AB-EP-20 in molar ratio of epoxy group to amine hydrogen 1.1∶1 at room temperature for 3 h and then 60 ℃ for 3 h, the cured film exhibited the optimum properties with flexibility 1 mm, pencil hardness 2 H, adhesion 1, impact resistance ≥50 kg·cm, water-resistance(25 ℃)≥7 d and alcohol-resistance ≥30 d respectively.
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    Ultra-violet Spectrophotometric Determination of Triterpenoidic Acid in the Stems and Leaves of Melaleuca leucadendra
    FAN Chao-jun;BAO Chang-yu;BI He-ping;CHEN Zhan-juan
    2011, 31 (4):  75-78. 
    Abstract ( 1021 )   PDF (680KB) ( 683 )   Save
    The total content of triterpenoidic acid in the stems and leaves of Melaleuca leucadendra Linn.was determined using 5 % vanillin-acetic acid and perchloric acid as color system. Ursolic acid had a better linear relationship in the range of 0.20-1.60 mg/L and its regression equation was A=0.154 8C+0.028 6(r=0.999 3).The results showed that the total mass fractions of triterpenoidic acid in the stems and leaves of M. leucadendra were 1.096 % and 1.017 % respectively.
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    Diversities of Morphological Characteristics and Constituents of Pinus koraiensis Sieb.et Zucc. Seeds from Changbai Moutain and Xiaoxing'anling Areas
    WU Xiao-hong;LIU Ying-tian;GONG Jie;FENG Chen;WANG Xiao-tian;LI Jian-xin
    2011, 31 (4):  79-82. 
    Abstract ( 884 )   PDF (611KB) ( 751 )   Save
    Seminal morphological characteristics and constituents of Pinus koraiensis Sieb.et Zucc.seeds from Changbai Moutain and Xiaoxing'anling areas were studied.Results show that there are no siginificant difference among morphological characteristics of seed in two areas. The thousand seed mass was higher in Changbai Moutain, and kernel ratio of seed was higher in Xiaoxing'anling. The ash content was the same in these two areas. The least moisture content was 1.85 % in Xiaoxing'anling and 3.75 % in Changbai Moutain respectively. The oil content was 68.45 % in Xiaoxing'anling and all content beyond 65 % in these two areas. The protein content in Xiaoxing'anling was higher than that in Changbai Moutain. It was seen that in pine seed, not only amino acids and trace elements, but also contents of glutamic acid, aspartic acid, arginine, magnesium, zinc, manganese and other trace elements were high. Total amino acid content in Xiaoxing'anling was the highest, trace elements had little difference. The nutrient contents were rich in pine seed, as well. The results showed that the pine seeds from two areas in both morphology and constituents had no significant difference.
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    Chemical Constituents of Euonymus bockii Loes.
    HU Xin-ling;WANG Kui-wu
    2011, 31 (4):  83-86. 
    Abstract ( 944 )   PDF (524KB) ( 581 )   Save
    Chemical constituents of Euonymus bockii Loes.stem were isolated and purified by silica gel and sephadex LH-20 column chromatography. Their structures were elucidated by chemical and spectroscopic methods. Eleven compounds were identified as friedelin, 3-O-28-friedelanoic acid, 29-hydroxy-3-friedelanone, salaspermic acid, orthosphenic acid, wilforlide A, wilforlide B, 3-hydroxy-2-O-3-friedelen-29-oic acid, 3-hydroxy-2,24-dioxo-3-friedelen-29-oic acid, 20(29)-lupene-1β,3β-diol, and 20(30)-lupene-3β,29-diol.
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    Optimizing Conditions for Microwave-assisted Extraction of Cochineal Dye Using Response Surface Method
    GUO Yuan-heng;MA Li-yi;ZHENG Hua;ZHANG Hong;GAN Jin;LI Kai;TU Xing-hao
    2011, 31 (4):  87-92. 
    Abstract ( 939 )   PDF (1236KB) ( 751 )   Save
    Cochineal (Dactylopius coccus Costa) dye was extracted by microwave-assisted extraction with water. Effects of single-factor test on the yield of cochineal dye was carried out. The results show that for 5 g cochineal, the suitable conditions for extraction of dye are cochineal sample soaked in water for 40min before microwave treatment, ratio of liquid to material 7∶1(g∶mL), microwave power 700 W, microwave treatment time 60 s, and extract with water-bath at 75 ℃ for 40 min after microwave treatment. According to the single-factor test, the microwave-assisted extraction process parameters for extraction of cochineal dye were optimized using response surface method. The results show that the optimum parameters should be as follows: cochineal 5 g, ratio of liquid to material 7.5, microwave power 714 W, microwave treatment time 73 s. The extraction yield of conchineal dye is up to 7.30%. Under this conditon the reasonable extracting times is 12, the total yield of conchineal dye is 29.95 % and extraction yield is 95.13 %.
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    综述评论
    Research Progress on Preparation of Nano-size Carbon Sphere and Its Derivatives by Hydrothermal Method
    LI Min;SUN Jian;LI Wei;LIU Shou-xin
    2011, 31 (4):  93-101. 
    Abstract ( 882 )   PDF (1735KB) ( 693 )   Save
    Preparation methods of carbon sphere and its derivatives by hydrothermal approaches were reviewed. Raw materials and synthesis methods for preparation of nano-size carbon sphere with specific size and morphologies were summarized. The important applications and development prospect of carbon nanospheres were introduced.
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    Research Progress on Liriodenine
    LIU Yan-cheng;CHEN Zhen-feng;PENG Yan;LIANG Hong
    2011, 31 (4):  109-116. 
    Abstract ( 1421 )   PDF (1385KB) ( 817 )   Save
    The research progress on the phytochemistry, pharmacology, as well as antitumoral activity and mechanism of liriodenine was reviewed, which is a kind of typical oxoaporphine alkaloid. Liriodenine widely distributes in many natural plants of a series of families and genera, but the content is very low. Liriodenine exhibits extensive pharmacological activities, such as antitumoral, antibacterial, antifungal and trypanocidal activities, as well as anti-alzheimer's disease. It is seen that the significant antitumoral activity should be ascribed to the hyperconjugational planar structure of oxoaporphine as parent nucleus. Moreover, the pro-phase research progress as the rise of medicinal inorganic chemistry of liriodenine was also briefly introduced based on the authors' achieved research efforts. It could provide new strategy for the expanded research and application of liriodenine.
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    Review on Some Potential Plant Squalene Resources
    BI Liang-wu;ZHAO Zhen-dong;HAN Lu-lu;LI Da-wei
    2011, 31 (4):  102-108. 
    Abstract ( 1086 )   PDF (735KB) ( 705 )   Save
    The traditional resource of squalene is shark liver oil which has not been encouraged to be used. It is very important to search sustainable and safe natural resources, especially plant resources, for squalene preparation, research, and development instead of shark liver oil. The major plant squalene resources including fruits, seeds or oil of olive (Olea europaea L.), Camellia oleifera Abel., amaranth series (Amaranthus tricolor, A. cruentus, A. hypochon-driacus), Terminalia catappa L., Siraitia grosvenorii, Staphylea bumalda, etc., were introduced. Investigation of plant squalene resources could be contributed to the future research and utilization of squalene.
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    Review on the Mechanisms of the New Water-borne Preservatives in Treated Wood
    YU Li-li;GAO Jia;YANG Ying;CAO Jin-zhen;MA Xiao-jun
    2011, 31 (4):  117-122. 
    Abstract ( 1276 )   PDF (927KB) ( 792 )   Save
    The fixation mechanisms of the main water-borne preservatives in treated wood were reviewed. The fixation mechanism of copper-amine/ammonia based-wood preservative systems was ionic exchange reactions between the active ingredients in the preservative with the carboxyl groups and the hydroxyl groups in the wood lignin and hemicellulose. In the micro-copper wood preservative systems, the fixation mechanism is attributed to the stronger adhesive force between the higher molecular dispersing agent and cellulose. For the boron-based preservative system, the fixation mechanism is similar to the copper-based preservatives, but the borate could not be fixed in treated wood directly. Therefore the research of the active ingredient fixation in treated wood deals mainly about the following aspects: 1) improving the hydrophobic propertics of boron-based preservative-treated wood; 2) complexing with organic chemicals and generating stable compound fixed in treated wood.
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    Research Progress for Separation of Bio-oil by Column Chromatography
    YAN Cai-hui;ZHAO Wei;SHENG Chen;WU Xiao-na
    2011, 31 (4):  123-126. 
    Abstract ( 937 )   PDF (651KB) ( 742 )   Save
    The research progress of bio-oil separation using column chromatography as well as solvent extraction-column chromatography at home and abroad were introduced. The advantages and disadvantages of separation method for bio-oil using column chromatography were analyzed. It was pointed out that column chromatography may have protential application prospect for bio-oil separation in the future.
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